CN102515558B - Method for preparing transparent conductive carbon nano tube film with combination method - Google Patents
Method for preparing transparent conductive carbon nano tube film with combination method Download PDFInfo
- Publication number
- CN102515558B CN102515558B CN2011103709124A CN201110370912A CN102515558B CN 102515558 B CN102515558 B CN 102515558B CN 2011103709124 A CN2011103709124 A CN 2011103709124A CN 201110370912 A CN201110370912 A CN 201110370912A CN 102515558 B CN102515558 B CN 102515558B
- Authority
- CN
- China
- Prior art keywords
- carbon nano
- quartz substrate
- tube film
- film
- carbon nanotube
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002238 carbon nanotube film Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000000758 substrate Substances 0.000 claims abstract description 53
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000010453 quartz Substances 0.000 claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 38
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 36
- 238000004528 spin coating Methods 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000007921 spray Substances 0.000 claims abstract description 15
- 238000005507 spraying Methods 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims 2
- 239000012153 distilled water Substances 0.000 claims 1
- 229960004756 ethanol Drugs 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000002270 dispersing agent Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000004886 process control Methods 0.000 abstract 1
- 230000006835 compression Effects 0.000 description 8
- 238000007906 compression Methods 0.000 description 8
- 239000010408 film Substances 0.000 description 8
- 238000002834 transmittance Methods 0.000 description 8
- 238000000576 coating method Methods 0.000 description 7
- 238000007493 shaping process Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002071 nanotube Substances 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000001652 electrophoretic deposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000001241 arc-discharge method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
- Manufacturing Of Electric Cables (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
一种以组合法制备透明导电碳纳米管薄膜的方法，属于纳米材料技术领域。本发明采用石英玻片作为基体，用纯化后的碳纳米管和无水乙醇分别作为原料和分散剂，用组合法制备了平均厚度为纳米级的透明导电碳纳米管薄膜。具体步骤如下：将一定量碳纳米管加到无水乙醇中，超声波分散数小时，得到分散均匀的溶液；将其倒入压缩式喷雾器中，喷涂到石英基体表面上；将上述覆盖碳纳米管薄膜的石英基体放置到旋转涂膜机的吸盘上进行旋涂定型，干燥；再进行喷涂，旋涂定型，如此往复操作，即可获得均匀的透明导电碳纳米管薄膜。本发明的原料易得，成本低廉，能耗低。制备工艺简单，工艺控制简洁，制得的碳纳米管薄膜，均匀，透明导电，具有广泛的应用前景。The invention discloses a method for preparing a transparent conductive carbon nanotube film by a combined method, which belongs to the technical field of nanomaterials. The invention adopts quartz glass plate as matrix, uses purified carbon nanotube and absolute ethanol as raw material and dispersant respectively, and prepares a transparent conductive carbon nanotube film with an average thickness of nanometer by a combination method. The specific steps are as follows: add a certain amount of carbon nanotubes to absolute ethanol, and disperse them by ultrasonic waves for several hours to obtain a uniformly dispersed solution; pour it into a compressed sprayer and spray it on the surface of the quartz substrate; The quartz substrate of the film is placed on the suction cup of the spin coating machine for spin coating and setting, and then dried; then spraying, spin coating and setting, such reciprocating operations, can obtain a uniform transparent conductive carbon nanotube film. The raw materials of the invention are easy to obtain, low in cost and low in energy consumption. The preparation process is simple, the process control is simple, and the prepared carbon nanotube film is uniform, transparent and conductive, and has wide application prospects.
Description
技术领域 technical field
本发明涉及一种纳米材料技术领域的制备方法，具体是一种以组合法制备透明导电碳纳米管薄膜的方法。 The invention relates to a preparation method in the technical field of nanometer materials, in particular to a method for preparing a transparent conductive carbon nanotube film by a combined method.
背景技术 Background technique
碳纳米管具有独特的纳米结构，使其具有特异的电学性能，力学性能，光学性能以及磁学性能等，为其在众多领域的应用提供了广阔前景。 Carbon nanotubes have a unique nanostructure, which makes them have specific electrical properties, mechanical properties, optical properties and magnetic properties, etc., providing broad prospects for their application in many fields.
利用碳纳米管良好的导电性制备具有高透明性和导电性的碳纳米管薄膜材料，在显示技术、太阳能电池、电子器件以及光学器件等方面有着广阔的应用前景，特别是有可能做为替代铟锡氧化物薄膜ITO的首选材料。 Using the good conductivity of carbon nanotubes to prepare carbon nanotube film materials with high transparency and conductivity has broad application prospects in display technology, solar cells, electronic devices, and optical devices, especially as an alternative The material of choice for indium tin oxide thin film ITO.
现有碳纳米管薄膜的制备方法主要有干法和湿法。干法有化学气相沉积法。湿法主要是先把CNT分散在溶液中，再借助于各种成膜技术获得表面平整的CNT薄膜，如旋涂法，电泳沉积法，过滤法，电弧放电法等，液浇铸法，层-层吸附自组装法，电泳沉积法，电化学沉积法，自组装成膜法，浸渍涂布法，改性表面吸附法，过滤-转移法和LB技术等。所用的CNTs均为化学修饰的官能化的碳纳米管，其外侧壁上常常带有游离的羟基、羧基等活性基团，当作为电化学器件使用时，在电流的催化下，这些存在于CNTs表面上的游离活性基团易发生不可逆的氧化限制了其使用范围。另外这些方法在制备过程需要高温作用、表面活性剂、催化剂，设备昂贵，制备过程复杂。 The existing preparation methods of carbon nanotube films mainly include dry method and wet method. The dry method has chemical vapor deposition method. The wet method is mainly to disperse CNT in the solution first, and then obtain a smooth CNT film by means of various film-forming techniques, such as spin coating method, electrophoretic deposition method, filtration method, arc discharge method, etc., liquid casting method, layer- Layer adsorption self-assembly method, electrophoretic deposition method, electrochemical deposition method, self-assembly film formation method, dipping coating method, modified surface adsorption method, filtration-transfer method and LB technology, etc. The CNTs used are chemically modified functionalized carbon nanotubes, and their outer walls often have active groups such as free hydroxyl groups and carboxyl groups. When used as electrochemical devices, under the catalysis of the current, these exist in the CNTs The irreversible oxidation of free active groups on the surface limits its application range. In addition, these methods require high temperature action, surfactants and catalysts in the preparation process, expensive equipment and complicated preparation process.
发明内容 Contents of the invention
本发明在现有技术的基础上，提供一种以组合法制备透明导电碳纳米管薄膜的方法。具体是采用石英玻片作为基体，纯化后的碳纳米管和无水乙醇分别作为原料和分散剂，将两者混合得到分散均匀的溶液，采用压缩式喷雾器将其喷涂到干燥洁净的石英基体上，得到第一层含有溶剂的碳纳米管薄膜；然后将其放置到高速旋转的涂膜机的吸盘上进行旋涂定型，如此反复操作，该过程中分散剂自然挥发，或通过加热使分散剂挥发，即可得到均匀的平均厚度为50-400nm的透明导电碳纳米管薄膜，电阻率为100-700 Ω/sq，透光率达到80-89%。 On the basis of the prior art, the invention provides a method for preparing a transparent conductive carbon nanotube film by a combined method. Specifically, quartz glass is used as the substrate, purified carbon nanotubes and absolute ethanol are used as raw materials and dispersants respectively, and the two are mixed to obtain a uniformly dispersed solution, which is sprayed onto the dry and clean quartz substrate by a compressed sprayer , to obtain the first layer of carbon nanotube film containing a solvent; then place it on the suction cup of a high-speed rotating film coating machine for spin coating and setting, and so on, the dispersant is naturally volatilized during this process, or the dispersant Volatilize to obtain a uniform transparent conductive carbon nanotube film with an average thickness of 50-400nm, a resistivity of 100-700 Ω/sq, and a light transmittance of 80-89%.
本发明是通过以下技术方案实现的，本发明采用石英玻片作为基体，纯化后的碳纳米管和无水乙醇分别作为原料和分散剂，利用压缩式喷雾器将碳纳米管和无水乙醇形成的高度分散的碳纳米管溶液均匀地喷涂在基体上，接着将得到的薄膜基体放置到旋转涂膜机的吸盘上进行旋涂定型，伴随着有机溶剂挥发，直接形成碳纳米管薄膜。其中无水乙醇作为有机溶剂，能与碳纳米管容易形成高分散的溶液，在室温或加热条件下溶剂容易挥发。此外，在制备过程不需要使用粘结剂和催化剂、不需要高温作用，设备简易，制备过程简单，易于连续化操作。本发明所用的原料简单易得，成本低廉，能耗低。制备工艺简洁，得到均匀透明导电的碳纳米管薄膜，具有广泛的应用前景。 The present invention is achieved through the following technical proposals. The present invention adopts quartz glass slides as a substrate, purified carbon nanotubes and absolute ethanol as raw materials and dispersants respectively, and utilizes a compression sprayer to form carbon nanotubes and absolute ethanol. The highly dispersed carbon nanotube solution is uniformly sprayed on the substrate, and then the obtained film substrate is placed on the suction cup of the spin coating machine for spin coating and finalization. With the volatilization of the organic solvent, the carbon nanotube film is directly formed. Among them, absolute ethanol is used as an organic solvent, which can easily form a highly dispersed solution with carbon nanotubes, and the solvent is easy to volatilize at room temperature or under heating conditions. In addition, the preparation process does not require the use of binders and catalysts, does not require high temperature action, simple equipment, simple preparation process, and easy continuous operation. The raw materials used in the invention are simple and easy to obtain, with low cost and low energy consumption. The preparation process is simple, and a uniform, transparent and conductive carbon nanotube film is obtained, which has wide application prospects.
本发明主要包括以下步骤： The present invention mainly comprises the following steps:
(1)将0.1-10 mg直径为2-30 nm，层数为1-30层的碳纳米管，加到50-300 mL无水乙醇中，利用超声波分散24-48 h，得到分散均匀的溶液； (1) Add 0.1-10 mg of carbon nanotubes with a diameter of 2-30 nm and a layer number of 1-30 to 50-300 mL of absolute ethanol, and disperse them by ultrasonic waves for 24-48 h to obtain uniformly dispersed solution;
(2)采用压缩式喷雾器将碳纳米管溶液喷涂到干燥洁净的石英基体表面上，得到第一层含有溶剂的碳纳米管薄膜。具体包括以下步骤：(a)将步骤(1)得到的碳纳米管溶液倒入压缩式压缩式喷雾器中；(b)在室温下，保持压缩式喷雾器的喷嘴距离石英基体表面为5-30cm, 将其喷涂到干燥洁净的石英基体表面上，其中，石英基体可以水平放置、竖直放置或与水平面形成夹角α（0°> α> 90°）放置； (2) Spraying the carbon nanotube solution onto the surface of a dry and clean quartz substrate by using a compression sprayer to obtain a first layer of carbon nanotube film containing a solvent. It specifically comprises the following steps: (a) pouring the carbon nanotube solution obtained in step (1) into a compressed sprayer; (b) keeping the nozzle of the compressed sprayer at 5-30 cm from the surface of the quartz substrate at room temperature, Spray it on the surface of a dry and clean quartz substrate, where the quartz substrate can be placed horizontally, vertically or at an angle α (0°>α>90°) with the horizontal plane;
(3)对步骤(2)得到的碳纳米管薄膜进行旋涂。具体包括以下步骤：(a)将步骤(2)得到的薄膜基体放置到旋转涂膜机的吸盘上，进行旋涂定型, 旋转速度为2000-5000转/分，时间为5-120 s; (b)将旋涂后的样品置于室内使溶剂自然挥发，或者置于真空干燥箱内干燥，温度设为30-100℃，干燥时间为10-60 min，得到第一层碳纳米管薄膜； (3) Spin coating the carbon nanotube film obtained in step (2). It specifically includes the following steps: (a) place the film substrate obtained in step (2) on the suction cup of the spin coating machine, and perform spin coating and setting, the rotation speed is 2000-5000 rpm, and the time is 5-120 s; ( b) Place the spin-coated sample indoors to allow the solvent to volatilize naturally, or dry it in a vacuum oven at a temperature of 30-100°C and a drying time of 10-60 min to obtain the first layer of carbon nanotube film;
(4)对步骤(3)得到的薄膜进行喷涂和旋涂。具体包括以下步骤：(a) 将压缩式喷雾器中的碳纳米管溶液进行超声处理; (b)对步骤(3)得到的第一层碳纳米管薄膜再进行喷涂，旋涂（方法与步骤(2)和步骤(3)相同），如此往复操作50-500次，即可获得平均厚度为50-400 nm的均匀的透明导电碳纳米管薄膜。 (4) Spray coating and spin coating the film obtained in step (3). It specifically includes the following steps: (a) ultrasonically treating the carbon nanotube solution in the compression sprayer; (b) spraying and spin-coating the first layer of carbon nanotube film obtained in step (3) (method and step ( 2) Same as step (3)), so reciprocating 50-500 times, a uniform transparent conductive carbon nanotube film with an average thickness of 50-400 nm can be obtained.
本发明具有如下有益效果：本发明采用本课题组自制的碳纳米管作为原料，无水乙醇作为分散剂，成本低廉，对环境无污染；产物易于处理，收率高，设备简单，工艺简洁，能耗低，容易得到碳纳米管薄膜，并可根据需要，对得到的碳纳米管薄膜平均厚度可在50-400 nm之间任意调节。 The present invention has the following beneficial effects: the present invention adopts carbon nanotubes self-made by the research group as raw materials, and absolute ethanol as a dispersant, with low cost and no pollution to the environment; the product is easy to handle, high in yield, simple in equipment and simple in process, Low energy consumption, easy to obtain carbon nanotube film, and according to needs, the average thickness of the obtained carbon nanotube film can be adjusted arbitrarily between 50-400 nm.
具体实施方式 Detailed ways
本实施例是在发明技术方案为前提下进行实施，给出了详细的实施方式和过程，但本发明的保护范围不限于下述的实施例。 This embodiment is implemented on the premise of the technical solution of the invention, and detailed implementation methods and processes are given, but the protection scope of the present invention is not limited to the following embodiments.
实施例1 Example 1
将0.1 mg直径为2-5 nm，层数为1层的碳纳米管加到200 mL无水乙醇中，超声分散48 h，得到分散均匀的溶液A。将溶液A倒入压缩式喷雾器中，在室温下，保持压缩式喷雾器的喷嘴距离石英基体表面为30 cm，将溶液A喷涂到干燥洁净的水平放置的石英基体表面上，得到覆有碳纳米管薄膜的石英基体B；将B放置到旋转涂膜机的吸盘上进行定型，第一阶段旋转速度为2000转/分，旋转时间为10 s；得到覆有碳纳米管薄膜的石英基体C；将C置于干净的表面皿内，放入真空干燥箱，干燥温度设为30℃，保温30 min，得到覆有碳纳米管薄膜的石英基体D，再对D表面进行喷涂（压缩式喷雾器中的碳纳米管溶液每隔60 min 进行超声处理10 min），旋涂定型，干燥，如此往复操作50次，即可获得平均厚度为50-100 nm的均匀的透明导电碳纳米管薄膜，电阻700 Ω/sq，透光率达到89%。 Add 0.1 mg of carbon nanotubes with a diameter of 2-5 nm and 1 layer to 200 mL of absolute ethanol, and ultrasonically disperse for 48 hours to obtain a uniformly dispersed solution A. Pour solution A into a compressed sprayer. At room temperature, keep the nozzle of the compressed sprayer at a distance of 30 cm from the surface of the quartz substrate, and spray solution A onto a dry and clean horizontally placed surface of the quartz substrate to obtain a carbon nanotube-coated The quartz substrate B of the thin film; place B on the suction cup of the rotary coating machine for shaping, the first stage rotation speed is 2000 rpm, and the rotation time is 10 s; the quartz substrate C covered with the carbon nanotube film is obtained; Place C in a clean watch glass, put it into a vacuum drying oven, set the drying temperature to 30°C, and keep it warm for 30 minutes to obtain a quartz substrate D covered with a carbon nanotube film, and then spray the surface of D (in a compressed sprayer) The carbon nanotube solution is ultrasonically treated every 60 min for 10 min), spin-coated to shape, and dried, so that the reciprocating operation is performed 50 times to obtain a uniform transparent conductive carbon nanotube film with an average thickness of 50-100 nm and a resistance of 700 Ω /sq, the light transmittance reaches 89%.
实施例2 Example 2
将0.5 mg直径为5-10 nm，层数为2-5层的碳纳米管加到200 mL无水乙醇中，超声分散48 h，得到分散均匀的溶液A。将溶液A倒入压缩式喷雾器中，在室温下，保持压缩式压缩式喷雾器的喷嘴距离石英基体表面的距离为25 cm，将溶液A喷涂到干燥洁净的竖直放置的石英基体表面上，得到覆有碳纳米管薄膜的石英基体B；将B放置到旋转涂膜机的吸盘上进行定型，旋转速度为2500转/分，旋转时间为20 s；得到覆有碳纳米管薄膜的石英基体C；将C置于干净的表面皿内，放入真空干燥箱，干燥温度设为30℃，保温1 h，得到覆有碳纳米管薄膜的石英基体D，再对D表面进行喷涂（压缩式喷雾器中的碳纳米管溶液每隔50 min 进行超声处理10 min），旋涂定型，干燥，如此往复操作100次，即可获得平均厚度为55-150 nm的均匀的透明导电碳纳米管薄膜，电阻600 Ω/sq，透光率达到88%。 Add 0.5 mg of carbon nanotubes with a diameter of 5-10 nm and a layer number of 2-5 to 200 mL of absolute ethanol, and ultrasonically disperse for 48 h to obtain a uniformly dispersed solution A. Pour solution A into a compressed sprayer, and at room temperature, keep the nozzle of the compressed compressed sprayer at a distance of 25 cm from the surface of the quartz substrate, and spray solution A onto the surface of a dry, clean, vertically placed quartz substrate to obtain Quartz substrate B covered with a carbon nanotube film; place B on the suction cup of a rotary coating machine for shaping, the rotation speed is 2500 rpm, and the rotation time is 20 s; the quartz substrate C covered with a carbon nanotube film is obtained ; Place C in a clean watch glass, put it into a vacuum drying oven, set the drying temperature to 30°C, and keep it warm for 1 h to obtain a quartz substrate D covered with a carbon nanotube film, and then spray the surface of D (compression sprayer The carbon nanotube solution in the solution is ultrasonically treated every 50 min for 10 min), spin-coated to shape, and dried, and so reciprocated 100 times, a uniform transparent conductive carbon nanotube film with an average thickness of 55-150 nm can be obtained, and the resistance 600 Ω/sq, light transmittance reaches 88%.
实施例3 Example 3
将1 mg直径为5-10 nm，层数为2-5层的碳纳米管，加到无水乙醇200 mL中，超声分散24 h，得到分散均匀的溶液A。将溶液A倒入压缩式喷雾器中，在室温下，保持压缩式压缩式喷雾器的喷嘴距离石英基体表面为20 cm，将溶液A喷涂到干燥洁净的石英基体表面上（与水平面形成45°的夹角），得到覆有碳纳米管薄膜的石英基体B；将B放置到旋转涂膜机的吸盘上进行定型，旋转速度为3000转/分，旋转时间为30 s；得到覆有碳纳米管薄膜的石英基体C；将C置于干净的表面皿内，放入真空干燥箱，干燥温度设为50℃，保温30 min，得到覆有碳纳米管薄膜的石英基体D，再对D表面进行喷涂（压缩式喷雾器中的碳纳米管溶液每隔40 min 进行超声处理10 min），旋涂定型，如此往复操作150次，即可获得平均厚度为60-200 nm的均匀的透明导电碳纳米管薄膜，电阻500 Ω/sq，透光率达到87%。 Add 1 mg of carbon nanotubes with a diameter of 5-10 nm and 2-5 layers into 200 mL of absolute ethanol, and ultrasonically disperse for 24 h to obtain a uniformly dispersed solution A. Pour solution A into a compressed sprayer. At room temperature, keep the nozzle of the compressed compressed sprayer at a distance of 20 cm from the surface of the quartz substrate, and spray solution A onto the surface of a dry and clean quartz substrate (with a 45° clamp to the horizontal plane. Angle), to obtain the quartz substrate B covered with carbon nanotube film; place B on the suction cup of the spin coating machine for shaping, the rotation speed is 3000 rpm, and the rotation time is 30 s; Quartz substrate C; put C in a clean watch glass, put it into a vacuum drying oven, set the drying temperature to 50°C, and keep it warm for 30 minutes to obtain a quartz substrate D covered with a carbon nanotube film, and then spray the surface of D (The carbon nanotube solution in the compression sprayer is subjected to ultrasonic treatment for 10 minutes every 40 minutes), spin-coated and shaped, and reciprocated 150 times in this way, a uniform transparent conductive carbon nanotube film with an average thickness of 60-200 nm can be obtained , the resistance is 500 Ω/sq, and the light transmittance reaches 87%.
实施例4 Example 4
将2 mg直径为10-30 nm，层数为8-30层的碳纳米管，加到200 mL无水乙醇中，超声分散24 h，得到分散均匀的溶液A。将溶液A倒入压缩式喷雾器中，在室温下，保持压缩式压缩式喷雾器的喷嘴距离石英基体表面为15 cm，将溶液A喷涂到干燥洁净的水平放置的石英基体表面上，得到覆有碳纳米管薄膜的石英基体B；将B放置到旋转涂膜机的吸盘（旋转盘的加热温度为20℃）上进行定型，旋转速度为3500转/分，旋转时间为50 s；得到覆有碳纳米管薄膜的石英基体C；再对C表面进行喷涂（压缩式喷雾器中的碳纳米管溶液每隔60 min 进行超声处理10 min），旋涂定型，如此往复操作200次，即可获得平均厚度为70-250 nm的均匀的透明导电碳纳米管薄膜，电阻400 Ω/sq，透光率达到85%。 Add 2 mg of carbon nanotubes with a diameter of 10-30 nm and a layer number of 8-30 to 200 mL of absolute ethanol, and ultrasonically disperse for 24 h to obtain a uniformly dispersed solution A. Pour solution A into a compressed sprayer. At room temperature, keep the nozzle of the compressed compressed sprayer at a distance of 15 cm from the surface of the quartz substrate, and spray solution A onto a dry and clean horizontally placed surface of the quartz substrate to obtain a carbon-coated solution. The quartz substrate B of the nanotube film; place B on the suction cup of the rotary coating machine (the heating temperature of the rotary disc is 20°C) for shaping, the rotation speed is 3500 rpm, and the rotation time is 50 s; The quartz substrate C of the nanotube film; and then spray the surface of C (the carbon nanotube solution in the compression sprayer is subjected to ultrasonic treatment for 10 minutes every 60 minutes), spin coating and setting, and the average thickness can be obtained by reciprocating 200 times in this way It is a uniform transparent conductive carbon nanotube film of 70-250 nm, with a resistance of 400 Ω/sq and a light transmittance of 85%.
实施例5 Example 5
将3 mg直径为10-30 nm，层数为8-30层的碳纳米管，加到200 mL无水乙醇，超声分散24 h，得到分散均匀的溶液A。将溶液A倒入压缩式喷雾器中，在室温下，保持压缩式压缩式喷雾器的喷嘴距离石英基体表面为10cm，将溶液A喷涂到干燥洁净的垂直放置的石英基体表面上，得到覆有碳纳米管薄膜的石英基体B；将B放置到旋转涂膜机的吸盘（旋转盘的加热温度为30℃）上进行定型，旋转速度为4000转/分，旋转时间为60 s；得到覆有碳纳米管薄膜的石英基体C；再对C表面进行喷涂（压缩式喷雾器中的碳纳米管溶液每隔50 min 进行超声处理10 min），旋涂定型，如此往复操作300次，即可获得平均厚度为80-300 nm的均匀的透明导电碳纳米管薄膜，电阻300 Ω/sq，透光率达到84%。 Add 3 mg of carbon nanotubes with a diameter of 10-30 nm and a layer number of 8-30 to 200 mL of absolute ethanol, and ultrasonically disperse for 24 h to obtain a uniformly dispersed solution A. Pour solution A into a compressed sprayer. At room temperature, keep the nozzle of the compressed compressed sprayer 10 cm away from the surface of the quartz substrate, and spray solution A onto the surface of a dry, clean, vertically placed quartz substrate to obtain a carbon nanometer-coated solution. The quartz substrate B of the tube film; place B on the suction cup of the rotary coating machine (the heating temperature of the rotary disc is 30°C) for shaping, the rotation speed is 4000 rpm, and the rotation time is 60 s; The quartz substrate C of the tube thin film; then spray the surface of C (the carbon nanotube solution in the compression sprayer is subjected to ultrasonic treatment for 10 min every 50 min), spin coating and shape, and so reciprocate 300 times, the average thickness can be obtained. 80-300 nm uniform transparent conductive carbon nanotube film, with a resistance of 300 Ω/sq and a light transmittance of 84%.
实施例6 Example 6
将5 mg直径为10-30 nm，层数为8-30层的碳纳米管，加到200 mL无水乙醇中，超声分散24 h，得到分散均匀的溶液A。将溶液A倒入压缩式喷雾器中，在室温下，保持压缩式压缩式喷雾器的喷嘴距离石英基体表面为10 cm，将溶液A喷涂到干燥洁净的石英基体表面上（与水平面形成45°的夹角），得到覆有碳纳米管薄膜的石英基体B；将B放置到旋转涂膜机的吸盘（旋转盘的加热温度为20-50℃）上进行定型，旋转速度为4500转/分，旋转时间为80 s；得到覆有碳纳米管薄膜的石英基体C；将沉淀C置于干净的表面皿内，放入真空干燥箱，干燥温度设为30℃，保温10 min，得到覆有碳纳米管薄膜的石英基体D，再对D表面进行喷涂（压缩式喷雾器中的碳纳米管溶液每隔40 min 进行超声处理10 min），旋涂定型，如此往复操作400次，即可获得平均厚度为90-350 nm的均匀的透明导电碳纳米管薄膜，电阻200 Ω/sq，透光率达到83%。 Add 5 mg of carbon nanotubes with a diameter of 10-30 nm and a layer number of 8-30 to 200 mL of absolute ethanol, and ultrasonically disperse for 24 h to obtain a uniformly dispersed solution A. Pour solution A into a compressed sprayer. At room temperature, keep the nozzle of the compressed compressed sprayer at a distance of 10 cm from the surface of the quartz substrate, and spray solution A onto the dry and clean surface of the quartz substrate (with a 45° clamp to the horizontal plane. Angle), to obtain the quartz substrate B covered with carbon nanotube film; place B on the suction cup of the rotary coating machine (the heating temperature of the rotary disc is 20-50 ℃) for shaping, the rotation speed is 4500 rpm, and the The time was 80 s; the quartz substrate C covered with carbon nanotube film was obtained; the precipitate C was placed in a clean watch glass, put into a vacuum drying oven, the drying temperature was set at 30°C, and the temperature was kept for 10 min to obtain a carbon nanotube coated substrate C. The quartz substrate D of the tube film is sprayed on the surface of D (the carbon nanotube solution in the compression sprayer is subjected to ultrasonic treatment for 10 min every 40 min), and the spin coating is finalized. The average thickness can be obtained by reciprocating 400 times in this way. 90-350 nm uniform transparent conductive carbon nanotube film with a resistance of 200 Ω/sq and a light transmittance of 83%.
实施例7 Example 7
将10 mg直径为10-30 nm，层数为8-30层的碳纳米管加到200 mL无水乙醇中，超声分散24 h，得到分散均匀的溶液A。将溶液A倒入压缩式喷雾器中，在室温下，保持压缩式压缩式喷雾器的喷嘴距离石英基体表面为5 cm，将溶液A喷涂到干燥洁净的水平放置的石英基体表面上，得到覆有碳纳米管薄膜的石英基体B；将B放置到旋转涂膜机的吸盘上进行定型，旋转速度为5000转/分，旋转时间为100 s；得到覆有碳纳米管薄膜的石英基体C；将沉淀C置于干净的表面皿内，放入真空干燥箱，干燥温度设为40℃，保温1 h，覆有碳纳米管薄膜的石英基体D，再对D表面进行喷涂（压缩式喷雾器中的碳纳米管溶液每隔40 min 进行超声处理10 min），旋涂定型，如此往复操作500次，即可获得平均厚度为100-400 nm的均匀的透明导电碳纳米管薄膜，电阻100 Ω/sq，透光率达到80%。 Add 10 mg of carbon nanotubes with a diameter of 10-30 nm and a layer number of 8-30 to 200 mL of absolute ethanol, and ultrasonically disperse for 24 h to obtain a uniformly dispersed solution A. Pour solution A into a compressed sprayer, and at room temperature, keep the nozzle of the compressed compressed sprayer at a distance of 5 cm from the surface of the quartz substrate, and spray solution A onto a dry and clean horizontally placed surface of the quartz substrate to obtain a carbon-coated The quartz substrate B of the nanotube thin film; B is placed on the suction cup of the rotary coating machine for shaping, the rotation speed is 5000 rpm, and the rotation time is 100 s; the quartz substrate C covered with the carbon nanotube thin film is obtained; C is placed in a clean watch glass, put into a vacuum drying oven, the drying temperature is set at 40°C, and kept for 1 h, the quartz substrate D covered with a carbon nanotube film is sprayed on the surface of D (carbon in a compressed sprayer The nanotube solution is ultrasonically treated every 40 min for 10 min), spin-coated, and reciprocated 500 times to obtain a uniform transparent conductive carbon nanotube film with an average thickness of 100-400 nm and a resistance of 100 Ω/sq. The light transmittance reaches 80%.
Claims (8)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103709124A CN102515558B (en) | 2011-11-21 | 2011-11-21 | Method for preparing transparent conductive carbon nano tube film with combination method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103709124A CN102515558B (en) | 2011-11-21 | 2011-11-21 | Method for preparing transparent conductive carbon nano tube film with combination method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102515558A CN102515558A (en) | 2012-06-27 |
| CN102515558B true CN102515558B (en) | 2013-12-04 |
Family
ID=46286703
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011103709124A Active CN102515558B (en) | 2011-11-21 | 2011-11-21 | Method for preparing transparent conductive carbon nano tube film with combination method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102515558B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014141279A1 (en) * | 2013-03-14 | 2014-09-18 | Vulcan Automotive Industries Ltd | Process for obtaining mixtures of carbon nanotubes in solid or viscous matrices |
| CN105016627A (en) * | 2015-06-10 | 2015-11-04 | 青岛科技大学 | Carbon nano-tube conductive glass preparation method |
| CN116351683B (en) * | 2023-03-17 | 2023-12-22 | 福建迈特富科技发展有限公司 | Preparation method and device of carbon nanotube film |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1671481A (en) * | 2002-05-21 | 2005-09-21 | 艾考斯公司 | Method for patterning carbon nanotube coating and carbon nanotube wiring |
| CN1962429A (en) * | 2006-11-27 | 2007-05-16 | 西南交通大学 | Preparation method of pure nano-carbon tube film |
| KR20080107814A (en) * | 2007-06-08 | 2008-12-11 | 한국기계연구원 | Single layer coating structure of carbon nanotube and manufacturing method thereof |
| JP2010108986A (en) * | 2008-10-28 | 2010-05-13 | Hitachi Chem Co Ltd | Material forming gate insulating film layer, field effect transistor and process for fabricating field effect transistor |
-
2011
- 2011-11-21 CN CN2011103709124A patent/CN102515558B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1671481A (en) * | 2002-05-21 | 2005-09-21 | 艾考斯公司 | Method for patterning carbon nanotube coating and carbon nanotube wiring |
| CN1962429A (en) * | 2006-11-27 | 2007-05-16 | 西南交通大学 | Preparation method of pure nano-carbon tube film |
| KR20080107814A (en) * | 2007-06-08 | 2008-12-11 | 한국기계연구원 | Single layer coating structure of carbon nanotube and manufacturing method thereof |
| JP2010108986A (en) * | 2008-10-28 | 2010-05-13 | Hitachi Chem Co Ltd | Material forming gate insulating film layer, field effect transistor and process for fabricating field effect transistor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102515558A (en) | 2012-06-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhao et al. | Spray deposition of steam treated and functionalized single-walled and multi-walled carbonnanotube films for supercapacitors | |
| CN104681645B (en) | A kind of method preparing composite transparent conductive electrode based on metal grill and metal nanometer line | |
| CN103072976B (en) | Transfer method of graphene or oxidized graphene thin film | |
| CN107113920A (en) | Transparent planar heat producing body | |
| CN103232033B (en) | Method for covering surface of substrate with graphene transparent film | |
| CN100511727C (en) | Method for manufacturing dye sensitized nano crystal solar cell photo-anode membrane | |
| CN106848494B (en) | A kind of simple preparation method of carbon auto-dope nano carbon nitride film electrode | |
| CN105555708A (en) | Carbon nanotubes, dispersion liquid thereof, carbon nanotube-containing film and composition material | |
| CN106782891A (en) | The preparation method of metal oxide compound silver nanometer line transparent conductive film | |
| CN103700430B (en) | A kind of conductive film being distributed in order and its manufacture method | |
| CN104626680B (en) | A kind of composite black titanium deoxid film and preparation method thereof | |
| CN104148655B (en) | A kind of environment-friendly preparation method thereof of flake silver powder | |
| CN103710685B (en) | A kind of spraying method directly preparing transparent graphene conductive film on a flexible substrate | |
| CN102581267A (en) | Silver-graphene composite material and method for conveniently producing silver-graphene composite material | |
| CN101654784A (en) | Method for preparing flexible carbon nano tube transparent conductive thin-film material and electrodeposition device | |
| CN104313549A (en) | Making method of graphene-based film with automatic cleaning function | |
| CN107705884A (en) | A kind of electrically conducting transparent paper based on nano silver wire and preparation method thereof | |
| CN102515558B (en) | Method for preparing transparent conductive carbon nano tube film with combination method | |
| CN103236323A (en) | Preparation method of composite transparent conductive film of metal nanowires and metallic oxides | |
| CN113963844B (en) | Flexible silver nanowire-based composite transparent film heater and preparation method thereof | |
| CN110364628A (en) | A kind of mixed dimension flexible transparent electrode and its preparation method and application | |
| CN101847459A (en) | Composite carbon nanotube conductive thin film and preparation method and preparation device thereof | |
| CN103627219B (en) | Organic modification method of Halloysite nanotubes | |
| CN107946467A (en) | A kind of polymer solar battery based on multiple light trapping structure and preparation method thereof | |
| CN102881458A (en) | Preparation method of graphene composite titanium dioxide slurry |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20180904 Address after: 100195 No. 116, building 2, B District, 80, Xing Shi Kou Road, Haidian District, Beijing. Patentee after: BEIJING XUJIANG TECHNOLOGY Co.,Ltd. Address before: 341000 Hongqi Avenue, Zhanggong District, Ganzhou, Jiangxi 86 Patentee before: Jiangxi University of Science and Technology |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20231130 Address after: 455000 Southwest corner of the intersection of No. 8 Road and No. 3 Road in Zhongyuan High tech Development Zone, Beiguan District, Anyang City, Henan Province Patentee after: Henan Yufeng Power Technology Co.,Ltd. Patentee after: TUNGHSU TECHNOLOGY GROUP Co.,Ltd. Address before: 100195 No. 116, building 2, B District, 80, Xing Shi Kou Road, Haidian District, Beijing. Patentee before: BEIJING XUJIANG TECHNOLOGY Co.,Ltd. |